Method of producing an aroma concentrate and the products obtained thereby

ABSTRACT

A method of producing aroma concentrates by smoking a meaty substance and then extracting with an organic solvent for the smoke flavor produced.

United States Patent Moller [54] METHOD OF PRODUCING AN AROMACONCENTRATE AND THE PRODUCTS OBTAINED THEREBY [72] Inventor: Hans G.Moller, 345 Holzminden, Hasenrecke 10, Germany [22] Filed: Feb. 16, 1970[21] Appl. No.: 11,881

[5 1] Int. Cl. ..A23l 1/26 [58] Field of Search ..99/l40 R, 110, 22,229, 3

[ 51 May 16, 1972 [56] References Cited UNITED STATES PATENTS 2,722,48211/1955 Betts ..99/140 Primary Examiner-Morris O. Wolk AssistantExaminer-Warren Bovee Attorney-Browdy and Neimark 5 7] ABSTRACT A methodof producing aroma concentrates by smoking a meaty substance and thenextracting with an organic solvent for the smoke flavor produced.

23 Claims, N0 Drawings METHOD OF PRODUCING AN AROMA CONCENTRATE AND THEPRODUCTS OBTAINED THEREBY The present invention relates to methods forthe production of aroma concentrates. More particularly the inventionrelates to aroma concentrates with the odor and taste of smoked baconand smoked ham. Such concentrates are, for example, suitable forflavoring foodstufis, animal feedstuff, and pesticides. They can also beused for other purposes, for instance for providing a scent.

The preserving of meat goods by smoking is amongst the oldest methods ofpreservation. Such smoking fulfills several purposes simultaneously,namely, preservation, coloration, and flavoring. In the present daystate of technology the preserving of meat products plays acomparatively small role as compared with flavoring the goods, for otherfoodstuffs, for example cheese, which have good keeping qualities arealso smoked.

In the preparation of foodstuffs, the addition of smoked food materials,particularly smoked bacon and smoked ham endow the foodstuff with aspecific taste, which may be highly esteemed by the consumer. Thesetaste components have up to now only been added by the direct additionof smoked meat products because there was no commercially availablenatural aroma concentrate. The provision of such an aroma concentrateforms one object of the invention which relates to natural smoked goodsaroma concentrates and methods for producing them.

The advantages that can be provided by an aroma concentrate inaccordance with the invention over previously conventional smoked goodsproducts lie on the one hand in the concentration itself and on theother in the possibilities of handling and using the concentrate. Theconcentrate can be readily standardized within certain limits as regardsstrength, yield, and flavor impression. It can be made with allsubstances necessary for flavoring and without ballast materials. Itthus enables the desired flavor to be produced, for instance infoodstuffs, without any change in consistency.

An aroma concentrate in accordance with the invention can be produced ina sterile condition and can also be incorporated in products which wouldbe spoiled by the addition of smoked bacon or smoked ham products.Finally the concentrate can be readily metered out and thus rationalizesoperations connected with the flavoring of a large number of differentsubstances, for example, foodstuffs in industry or in the home. It isnot necessary to explain in detail that in the case of the use of asmoked ham aroma concentrate it is not necessary to spend the time andtrouble necessary for smoking the material to be flavored and theassociated technological difficulties no longer arise.

Several different methods of smoking meat goods and other foodstufis areknown which all lead to the same result. For example smoking can becarried out in peat smoke with moderate smoke currents, or the smokingcan be carried out over a period of about 3 weeks in the case of ham andsausages with long keeping qualities. Industrial rapid smoking processesuse concentrated smoke at 12 to 80 C., the smoking period being lessthan 8 days. A further method makes use of smoke which is produced withthe help of super-heated steam so that there is a rapid smoking of thegoods. The preferred woods used for smoke production are oak, beech,hickory, and other hard woods. Aromatic plants may be added. The smokeproducing material has a moisture content of to 30 percent. Smolderingcombustion is carried out with an excess of atmospheric oxygen eitherdirectly or in an industrial plant constructed for the purpose. Theprecise method of smoking is, however, not essential to the presentinvention in the sense that any smoking process can be used.

It has been found that the aroma of smoked goods, such as smoked ham andsmoked bacon, can be obtained as an extract and concentrated if a smokedproduct produced in accordance with one of the above methods or anothermethod is extracted with a low boiling point solvent which may then bedistilled off. It has also been found that smoked ham aroma can beobtained as a steam distillate by treating the smoked product or theextract with steam and condensing the product which comes over in thesteam distillation. This distillate is then extracted with a low boilingpoint solvent and finally the solvent is distilled off from the extractproduced. The extracted solutions are preferably filtered beforedistilling off the solvent.

In many cases it is convenient to allow a mellowing or fermentation timebetween smoking of the foodstuff and extraction or steam distillation.Good results have been obtained with a fermentation time of 2 to 4 days,for instance 3 days, at normal room temperature. It is, however, alsopossible to carry out the fermentation at about C., in which case aperiod of time of 2 to 4 hours, for instance 3 hours is sufficient. Thisfermentation brings about a heightening of the flavor and taste so as toresemble the flavor of smoked bacon in the case of smoked products, sucha flavor only being obtained otherwise by the use of cold smoke, that isto say smoke between l0 and 40 C. and a considerable period of time. Inthe case of the use of smoke at a higher temperature this fermentationcan be dispensed with. It can also be dispensed with in the case ofsmoking fish meat.

A smoked ham aroma concentrate obtained in this manner has the fullflavor and taste of fresh ham which is obtained by smoking ham meat. inaccordance with the fat content of the products to be smoked and thesmoking temperature, extracts and concentrates are obtained whichpossess the savor and taste of fresh smoked ham, bacon and crackling.The concentrate obtained differs from pure condensed smoke as regardsits specifically smoked meat character. Such shades of taste could notbe obtained previously with any type of smoke concentrate.

Since smoking of meat in the first phase constitutes an absorption, ithas been found useful to increase the surface of the product to besmoked by chopping it up. The smoking of the chopped up meat mass isthen carried out, conveniently, using turbulent smoke, that is to say,smoke as produced by conventional smoke generators using blowers orfans.

It has been found surprisingly that the smoked and extracted meat masscan be smoked again after a drying process. However, in this case it isalways necessary to arrange for a fermentation period to occur beforethe renewed extraction.

The method in accordance with the invention can also be carried outcontinuously wherein, for example, chopped and predried meat wasteproducts are smoked in an inclined rotating drum continuously with apre-set residence or treatment time, following which the products arecontinuously removed, possibly subjected to a fermentation and thencontinuously extracted. The smoked and extracted meat mass can then berecirculated to the charging end of the smoking drum, possibly afterdriving off the solvent. if this continuous method is repeated with twoor more circuits of the material, the second and each following smokingstage should be followed by a fermentation stage. The fermentation ispreferably carried out in a zone following the smoking drum, where thesmoked material is freed from smoke. For the continuous method it hasbeen found particularly convenient to employ a short durationfermentation at a high temperature, for example 3 hours at 100 C., inorder to make the course of the process as rapid as possible.

The aroma concentrate obtained in accordance with the invention is aliquid and can readily be incorporated into materials such as sauces,soups, meat goods and fish, and also in cheese together with othermaterials. Alternatively, the concentrate can be applied to the surfaceof the material to be flavored. No substantial dilution of the materialto be flavored occurs in this case since 1 to 6 grams of concentrate aresufficient for treating 100 kilograms of finished products. Theflavoring of, for example, foodstuffs can be carried out directly withthe concentrate. However, the concentrate can also be applied in theform of a solution or suspension, for example in water, acidic liquidssuch as vinegar, alcohol, edible oils, fat, oil-water emulsions and/orother physiologically unobjectionable solvents or liquids. Thesuperficial application of the concentrate to solid base materials canbe carried out by spraying or dipping, for instance, of the material tobe flavored.

The novel aroma concentrate in accordance with the invention is alsocompletely sound as regards health aspects since it is produced fromsmoked foodstuffs which are themselves free to be eaten. It is knownthat in smoked products carcinogenic materials are produced which inpart become precipitated on the food material. Smoked products producedby longestablished methods after smoking with peat have a 3,4-benzpyrenecontent of l3 micrograms (Mg) per kilogram of smoked product. in thecase of the use of smoke producers which yield a cleaned smoke, forexample by scrubbing the smoke, the content limit is 0.2 to 0.3micrograms of 3,4-benzpyrene per kilogram of smoked material. Tests witha concentrate in accordance with the present invention obtained byextracting smoked goods with methylene chloride, filtration of theextract and evaporation of the solvent have shown that the concentrationof 3,4-benzpyrene in the flavored final product only amounted to 0.0005ppb. This quantity is practically negligible. In the case of enrichmentof the smoked ham aroma concentrate by steam distillation of the smokedmaterial and extraction of the distillate, or steam distillation of thesolvent extract and subsequent renewed extraction of the steamdistillate, there is an additional purifying effect. An aromaconcentrate obtained in such a manner is practically completely free ofbenzpyrene.

Preferred embodiments of the method in accordance with the invention inwhich an aroma concentrate is produced from meat, fish, their wasteproducts or preparations made from them which are smoked and extractedwith an organic solvent for the aroma from the smoked meat or fish,after which the solution is filtered if necessary, incorporate thefeature that a low boiling point solvent is used, more particularly ahalogenated hydrocarbon with a boiling point not exceeding 100 C. orpreferably below 60 C., or lower alkanols with one to four carbon atoms.

Methylene chloride can be used to make possible a particularly rapidextraction and is preferred for industrial application if a fat contentin the final product is not found inconvenient. Should a fat content beundesired, the extract can be subjected to steam distillation and thenextracted afresh.

If it is desired to avoid the extraction of fat in the course of theprocess, the use of lower alcohols with one to four carbon atoms ispreferred, ethanol being used if the alcoholic extract is to be useddirectly. It is naturally not possible to use highly water solublealcohols for the extraction of the steam distillate since there wouldthen be no phase separation.

Preferably the organic solvent used for the extraction is completelydistilled off. In the case of subsequent steam distillation it ispossible, if there is a sufficient difference in boiling points betweenthe organic solvent and the water, to carry out the steam distillationin such a manner that, firstly, the extraction solvent is driven off andthen a steam fraction is caught. If substantial quantities of the aromahave already been driven off with the organic solvent, the same organicsolvent can be used subsequently for the extraction of the steamdistillate in order to avoid losses of aroma concentrate.

Steam distillation of smoked products and the extraction of the steamdistillate are preferred if a practically completely fat-free and verypure aroma concentrate is required. Should fat-containing extracts haveto be converted into particularly pure extracts without any fat, steamdistillation of the organic solvent extracted and subsequent renewedextraction are recommended.

If an aroma with a pronounced smoked bacon character is desired, the useof a mellowing time of either 2 to 4 days at normal temperature or 2 to4 hours at about 100 C. is preferred.

For industrial applications the method is preferably carried outcontinuously, as has already been explained. In this case the materialintroduced into the smoking chamber should be capable of being poured,in the sense that solid particles can be poured, and not agglomerated.This can be achieved by a suitable pro-drying stage.

The invention is now explained with reference to the following examples:

EXAMPLE 1 10 kg of chopped unsmoked bacon rind were smoked using smokefrom a conventional smoke producer, the smoking temperature being 70 toC. and the water vapor content being approximately 20 to 30 percent.When the smoking time had elapsed, the product was divided up into twoequal parts which were treated in accordance with the following workingprocedures (a) and (b):

a. The part (a) was treated two times in a known manner with three timesits volume of diethyl ether with vigorous stirring for half an hour eachtime at 35 C. The organic phase was decanted and filtered and thesolvent distilled off carefully from the remaining aroma concentrate.

b. The part (b) was subjected for 60 minutes to steam distillation. Thedistillate was extracted by shaking with three portions of diethylether, the total quantity of ether being 400 ml. The organic phases werebulked and the solvent was distilled off carefully.

The product produced by the procedure (b) was practically free of fatand was approximately ten times more concentrated with respect to aromathan the product in accordance with the working method (a). Bothproducts could be diluted 50,000 to 500,000 times to yield,nevertheless, a good smoke savor and taste, which resembles the flavorof crackling.

EXAMPLE 2a The working procedure (a) of example I was repeated withethanol and methylene chloride respectively, the other particulars ofthe method being left unchanged. The products were practically identicalwith those of example la, but the fat content of the extract obtainedwith ethanol was very low.

EXAMPLE 2b In accordance with the working procedure (b) of example 1 thesteam distillate was extracted with three times its volume of petroleumether (boiling point range 50 to 70 C.), ethyl acetate and methylenechloride respectively. The products obtained were practically identicalto those obtained in the procedure (b) of example 1.

EXAMPLE 3 In a further trial, the products obtained in accordance withexample la and example 2a were subjected, after evaporating off theorganic solvent using a vacuum as produced by a water-jet filter pump,to steam distillation lasting for 1 hour. The steam distillate was takenup in three tests respectively with 300 ml. diethyl ether, 500 ml,methylene chloride and 500 ml. petroleum ether (boiling point range 50to 70 C.

After careful evaporation of the solvents using a vacuum sufficient toensure that a temperature of 50 C. was not exceeded, very pure andpotent concentrates were obtained which were practically free of fat andbenzpyrene. These aroma concentrates could be diluted 500,000 times.

EXAMPLE 4 10 kg of pigs ears were smoked with smoke from a smokegenerator at 30 to 40 C. This smoked product was allowed to rest for 3days at ambient temperature for fermentation and then treated inaccordance with the working procedures (a) and (b) of example 1, theextraction in both cases being carried out with double the quantity ofmethylene chloride using a Soxhlet extraction apparatus. Both extractsyield the same aroma which, after dilution as described in example 1,tastes and smells like well smoked ham.

EXAMPLE 5 3.5 kg of meat waste products, consisting mostly of bellycuts, were smoked with cold smoke at to C. After fermentation lastingfor 3 hours at 100 C. the smoked material was treated in accordance withprocedures (a) and (b) of example 1, 7 kg of methylene chloride beingused for extraction in each case. The extraction time lastedapproximately 3 hours. After dilution both extracts provided a verysatisfactory smoked ham aroma.

EXAMPLE 6 5.5 kg of meat waste, consisting mostly of unsmoked baconrind, were smoked using smoke produced by super-heated steam and woodchips. The smoked product was divided up as described in example 1 intotwo parts treated in accordance with procedures (a) and (b) ofexample 1. For the extraction in the method (a) Soxhlet apparatus usewas made of 10 kg of i'sopropanol while in the case of method (b) 5 kgof 1,2- dichloroethylene were used as an extraction solvent. Theconcentrate obtained in accordance with the two methods (a) and (b) hada smoke character which in flavor was more like that of crackling.

EXAMPLE 7 The extract residue and the residue subjected to steamdistillation obtained in the procedures (a) and (b) of example 4 andequal in weight each to 5 kg were dried and then smoked again at 30 to40 C. After the termination of smoking the product was left 8 days atambient temperature (approximately 16 to 18 C.) for fermentation. Theneach of the two 5 kg charges were processed as in the procedures (a) and(b) of example 1, methylene chloride being used for extraction in EACHcase. The concentrates obtained in this manner smelled and tasted alsolike ham.

EXAMPLE 8 Example 4 was carried out with 10 kg of fish waste as producedin preserving sardines, without, however, the use of a fermentationperiod. Both the working procedures (a) and (b) provide an aromaconcentrate which had a pronounced flavor of smoked fish.

EXAMPLES OF USE:

A. The product of the working procedure (a) of example 1 in a quantityequal to 15 g. was incorporated in 100 kg offresh liver sausage filling.The sausage produced from the filling had the flavor of smoked liversausage. In the case of the product of the procedure (b) of example 1the same flavor character was obtained using 2 g. of aroma per 100 kg ofliver sausage filling.

B. 5 g. of the product of example 4a was used in 100 kg of pea soup soas to endow the soup with the smell and taste of a soup cooked with hamor bacon.

C. 50 kg of poison bait wheat as supplied in trade for pest destruction,was wetted with a solution of 7.5 g. of the product of example 6a in lliter methylene chloride with thorough mixing. The solvent was allowedto evaporate. The bait wheat had a smell like that of crackling and wastaken more readily by mice and rats than wheat bait which had not beenso treated.

The same preparation can be carried out with 3 g. of the product ofexample 8b to yield a good poison bait.

D. 1.5 g. of the aroma concentrate in accordance with the procedure (a)of example 1 were worked into 50 kg of steamed, mashed potatoes. Thepotatoes were then mixed with 50 kg of rye bran. After mixing to makethe mass homogenous, extrusion to make pellets was carried out. Thepellets had a smell and taste of crackling and were suitable as dogfood. Conventional mineral and vitamin materials can be incorporated.

E. In order to endow leather with the odor of Russian leather, theproduct of example 1 (procedure (b)) was dissolved in a suitablequantity of water, or more conveniently,

an organic solvent with a low boiling point, and sprayed onto theleather, so that 10 to 100 ppm of the product was added to the leather.

It will be obvious to those skilled in the art that various changes maybe made without departing from the scope of the invention and theinvention is not to be considered limited to what is described in thespecification.

What is claimed is:

l. A method for producing an aroma concentrate comprising smoking ameaty substance, extracting with an organic solvent for the smoke flavorproduced, and after extraction filtering the solution.

2. A method in accordance with claim 1 wherein the substance is meat orfish.

3. A method in accordance with claim 1 wherein the sub stance is a meator fish waste product.

4. A method in accordance with claim 1 wherein the substance is a meator fish containing product.

5. A method in accordance with claim 1 wherein the smoked product issubjected to steam distillation and the distillate produced is extractedwith an organic solvent.

6. A method in accordance with claim 1 wherein the aroma extract issubjected to steam distillation and the resulting distillate is againextracted with organic solvent.

7. A method in accordance with claim 6 wherein the organic solvent isremoved before the steam distillation.

8. A method in accordance with claim 1 wherein after smoking the productis allowed to mellow before the aroma is removed.

9. A method in accordance with claim 1 wherein the organic solvent usedis distilled partially or totally from the solution of the aromasubstance.

10. A method in accordance with claim 1 wherein the surface of thesubstance to be smoked is increased by chopping up the substance.

11. A method in accordance with claim 10 wherein the material is driedbefore smoking.

12. A method in accordance with claim 1 wherein the smoke for thesmoking of the substance has a temperature between 10 and C. and a watervapor content of 10 to 97 percent.

13. A method in accordance with claim 12 wherein the smoke is producedfrom wet wood and is used at a temperature between 12 to 35 C. and awater vapor content of 20 to 40 percent.

14. A method in accordance with claim 13 wherein the smoke used forsmoking the substance is produced from a hard wood.

15. A method in accordance with claim 14 wherein the wood for producingthe smoke is beech, oak or hickory.

16. A method in accordance with claim 1 wherein the smoking is carriedout using turbulent smoke.

17. A method in accordance with claim 1 wherein aroma is removed fromthe substance, and the substance is again smoked and then aroma furtherremoved.

18. A method in accordance with claim 17 which is carried outcontinuously.

19. A method in accordance with claim 1 wherein the organic solvent usedas extraction solvent has a boiling point below 100 C.

20. A method in accordance with claim 19 wherein the solvent has aboiling point below 60 C.

21. A method in accordance with claim 19 wherein a low boiling pointhalogenated hydrocarbon is used as the solvent.

22. A method in accordance with claim 19 wherein a lower alcohol withone to four carbon atoms is used as extraction solvent.

23. An aroma concentrate produced by the method of claim 1.

2. A method in accordance with claim 1 wherein the substance is meat orfish.
 3. A method in accordance with claim 1 wherein the substance is ameat or fish waste product.
 4. A method in accordance with claim 1wherein the substance is a meat or fish containing product.
 5. A methodin accordance with claim 1 wherein the smoked product is subjected tosteam distillation and the distillate produced is extracted with anorganic solvent.
 6. A method in accordance with claim 1 wherein thearoma extract is subjected to steam distillation and the resultingdistillate is again extracted with organic solvent.
 7. A method inaccordance with claim 6 wherein the organic solvent is removed beforethe steam distillation.
 8. A method in accordance with claim 1 whereinafter smoking the product is allowed to mellow before the aroma isremoved.
 9. A method in accordance with claim 1 wherein the organicsolvent used is distilled partially or totally from the solution of thearoma substance.
 10. A method in accordance with claim 1 wherein thesurface of the substance to be smoked is increased by chopping up thesubstance.
 11. A method in accordance with claim 10 wherein the materialis dried before smoking.
 12. A method in accordance with claim 1 whereinthe smoke for the smoking of the substance has a temperature between 10*and 80* C. and a water vapor content of 10 to 97 percent.
 13. A methodin accordance with claim 12 wherein the smoke is produced from wet woodand is used at a temperature between 12* to 35* C. and a water vaporcontent of 20 to 40 percent.
 14. A method in accordance with claim 13wherein the smoke used for smoking the substance is produced from a hardwood.
 15. A method in accordance with claim 14 wherein the wood forproducing the smoke is beech, oak or hickory.
 16. A method in accordancewith claim 1 wherein the smoking is carried out using turbulent smoke.17. A method in accordance with claim 1 wherein aroma is removed fromthe substance, and the substance is again smoked and then aroma furtherremoved.
 18. A method in accordance with claim 17 which is carried outcontinuously.
 19. A method in accordance with claim 1 wherein theorganic solvent used as extraction solvent has a boiling point below100* C.
 20. A method in accordance with claim 19 wherein the solvent hasa boiling point below 60* C.
 21. A method in accordance with claim 19wherein a low boiling point halogenated hydrocarbon is used as thesolvent.
 22. A method in accordance with claim 19 wherein a loweralcohol with one to four carbon atoms is used as extraction solvent. 23.An aroma concentrate produced by the method of claim 1.